HRID1013120
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
Add 2-(3-chloropropyl)-2-phenyl-[1,3]dioxolane (38 g, 168 mmol) and potassium phthalimide (34.2 g, 184.4 mmol) to DMF (80 mL) and stir for 40 min at 150° C. Cool the reaction to RT, dilute with water (1 L) and extract the mixture with a mixture of EtOAc (500 mL) and hexanes (500 mL) and DCM (2 L). Dry (sodium sulfate), concentrate and recrystallize the solid from hot ethanol (600 mL). Filter and dry the residue under vacuum to isolate the title compound as a white solid (47.62 g, 84%).
WORKUP
后处理
- temperatureCool
- customthe reaction to RT
- extractionextract the mixture
- additionwith a mixture of EtOAc (500 mL) and hexanes (500 mL) and DCM (2 L)
- dry with materialDry (sodium sulfate)
- concentrationconcentrate
- customrecrystallize the solid from hot ethanol (600 mL)
- filtrationFilter
- customdry the residue under vacuum